基质固相分散萃取-HPLC分析番茄中6种农药残留

Determination of six pesticides residues in tomato by high performance liquid chromatography with matrix solid phase dispersion

建立番茄中6种农药的基质固相分散萃取-高效液相色谱(HPLC)检测方法。待测农药包括吡虫啉、啶虫脒、多菌灵、甲基硫菌灵、克百威和嘧霉胺。样品用乙腈作为提取溶剂经高速匀浆提取,并进一步由无水硫酸镁和乙二胺-N-丙基硅烷(PSA)净化后,采用Shiseido CAPCELL PAK MGⅡC18色谱柱分离,以甲醇、水和乙腈作为色谱分离的流动相进行梯度洗脱,紫外检测器测定外标法定量。结果表明:6种农药添加浓度0.05,0.10,0.20 mg/kg的回收率分别为71.5%～85.4%,78.9%～93.7%和87.8%～107.3%;相对标准偏差分别为7.47%～13.4%,5.32%～10.5%和4.32%～8.65%。说明该方法重现性好、灵敏度高,可以满足简便、快速、准确测定农药残留的要求,适合番茄中6种农药残留的同时检测及定量分析。

A method was established for the determination of imidacloprid,acetamiprid,carbendazim,thiophanate-methyl,carbofura and primigravida residues in tomato by using matrix solid phase dispersion-high performance liquid chromatography.The pesticide residues in the tomato samples were extracted by acetonitrile,cleaned up by MgSO4and ethylenediamine-N-propyl silyl（PSA）,and then analyzed by using high performance liquid chromatography ultraviolet detector with methyl alcohol,water and acetonitrile as gradient elution solvent,with Shiseido CAPCELL PAK MG ⅡC18as the analytical column.The average recoveries obtained from samples spiked with standards at concentration level 0.05,0.10and 0.20 mg/kg were in the range of 71.5% ～85.4%,78.9% ～93.7% and 87.8%～107.3%,respectively,with relative standard deviations（RSDs）of 7.47%～13.4%,5.32%～10.5% and 4.32%～8.65%.Apply this method on determining pesticide residues of tomato,which has more convenient operation,higher sensitivity,higher accuracy and better repeatability than others methods.This method is applicable to simultaneously confirm the residues of imidacloprid,acetamiprid,carbendazim,thiophanate-methyl,carbofura and primigravida in the tomato samples.